Process of preparing valuable compounds from the waste products obtained in the refining of cracked mineral oils



Apnl 2, 1935. w. VON PIOTROWSKI ET AL- 1,996,592

PROCESS OF PREPARING VALUABLE COMPOUNDS FROM THE WASTE PRODUCTS OBTAINEDIN THE REFINING OF CRACKED MINERAL OILS Filed'March 25, less PatentedApr. 2, 1935 v I UNITED STATES PATENT OFFICE PRooEss F PREPARINGVALUABLE COM- POUNDS FROM THE WASTE PRonUcTs OBTAINED IN THE REFINING 0FoRAoKEn MINERAL OILS Waelaw von Piotrowski and Jozef Winkler, Drohobycz,Poland ApplicationMarch 23, 1933, Serial no. 662,391

2 Claims. (Cl. 196-148) In U. S. Patent No. 1,869,231 we have describedThe apparatus used for carrying out the proca process for obtainingvaluable compounds from ess according to the invention comprises a stillthe waste products in the refining processes of I heated by any suitablemeans, for instance a cracked mineral oils, particularly crackedbenburner ID. The still is provided with three tubes,

6 zines with sulfuric acid. These products are a viz., an admission tubeland a tube 4 for intro- 5 mixture of olefines, diolefines, ketones,higher 211- ducing the oil to be treated, both tubes having cutcohols,sulfides, disulfides, mereaptanes, thiooff valves 12 and I4,respectively. Another pipe phenes and the like. Some fractions may beused 5 leads to a dephlegmator 6, said dephlegmator as insecticides orfungicides, furthermore as odorbeing connected by a tube 1 with a cooler8 and 10 izing substances for odorless gas and denaturiz- 'a receiver 9.In the pipe I a pressure regulating 10 v ingmeans for alcohol. valve 3is provided. The cooler 8 is provided with The above mentioned processcomprises. dilutwater inlet and outlet tubes H and I3.

ing the acid sludge with water or dilute caustic The p i arr d out as fl w alkali solutions, allowing the mixture to separate The oil isintroduced by the pipe 4 into the still into two layers, removing theoilylayer'after be- I and distilled with steam until all'the comv15 ingneutralized and'distilling it after drying. The pounds coming overbetween 50 C. and 280 C. V distillate coming over between 50 and 280 C.is have been driven off and collected. collected separately and mayafterwards be rec- Thereafter the steam admission valve 12 is tilled orfractionally distilled according to the declosed, the heating reducedand the pressure regsired end products. ulating valve 3 arranged in thepipe 3 near the 20 The residue of distillation is a product whichdephlegmator ,6 is slowly closed until the preshas about the followingproperties: sure in the still will amount to 6 atmospheres.

c The heating is slowly increased, whereupon a p fi gravlty at 15 C 960light distillate begins to escape through the Vlscoslty at c 98dephlegmator 6 and pipe I and cooler 8 t0 the 25 C Liquid receiver 9,The distillation is continued until the 9% specific gravity of thedistillate finally coming o'contents over amounts to 0.850.

What we claim is:--

This product was up to the present used as a 1. In a. process ofpreparing valuable comfuel, since another possibility of appllcation waspounds from the waste products obtained in the 5 tioned distillationresidue may be distilled with- 40 layer of the waste acid sludge asdescribed in 3; g gf a fi q fi asphalt refining of cracked mineral oilswith acid which g g y g 1 process comprises mixingthe wasteacid-containe and t s s the ing sludge with water and a dilute alkalinesoject of the present invention, that the above men- 111mm allowing themxture to separate into two layers, removing the upper oily layer,subjecting the same to steam distillation, thereby producing a pluralityof fractions collecting the fractions coming over between 50 C. and2800., the step of subjecting the residue of said steam distilla- 40 tionto a distillation by heating in the absence of steam undercracking-conditions thereby producing further quantities of distillates,coming over outsteam under cracking conditions, whereby it gives somemore distillates coming over between and 280 C. and having the samechemical nature as the products obtained by distilling the oily ourPatent 1,869,231.

By heating the said residue without steam, especially when pressure isapplied, a depolymero 7 ization occurs, yielding a mixture of productsrich g i gg f g g igfg g' claim 1, chariot- 45 m and in By this it isized thereb that the'distillates obtained by dism? the the Pmess tillingthe residue are joined with those obtained 7 scribed in Patent1,869,231, that the-yield in the steam distillation of the oily layer ofthe is almost a threefold one. waste acid s1udge v a In the accompanyingdrawing one embodiment WACLAW' v0 momowsxt j of the invention isillustrated. JOZEF

